TWI462791B - Method for forming nano sliver particles - Google Patents
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/056—Submicron particles having a size above 100 nm up to 300 nm
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/84—Manufacture, treatment, or detection of nanostructure
- Y10S977/895—Manufacture, treatment, or detection of nanostructure having step or means utilizing chemical property
- Y10S977/896—Chemical synthesis, e.g. chemical bonding or breaking
Description
本發明係關於一種奈米銀粒子的形成方法，且特別關於一種形成平均粒徑約50 nm-100 nm之奈米銀粒子的方法，特別是，此方法可應用於一放大之製程。The present invention relates to a method for forming nano silver particles, and more particularly to a method for forming nano silver particles having an average particle diameter of about 50 nm to 100 nm, and in particular, the method can be applied to an amplification process.
奈米銀對於微生物具有極強之氧化性，且因此奈米銀具有良好的抗菌或殺菌功效。而由於奈米銀具有良好的抗菌或殺菌功效，因此目前被廣泛應用來形成抗菌材料，例如奈米銀塗料等。Nano silver is extremely oxidizing to microorganisms, and thus nano silver has good antibacterial or bactericidal effects. Because nano silver has good antibacterial or bactericidal effects, it is widely used to form antibacterial materials, such as nano silver coatings.
然而，目前已有文獻證實，當奈米銀粒子尺寸小於30 nm時具有非常高的生物毒性，且其對人體與自然界的外在有利菌亦會產生傷害。因此歐美國家對於太小尺寸的奈米銀粒子的安全性已產生疑率。However, it has been confirmed in the literature that when the nano silver particle size is less than 30 nm, it has a very high biological toxicity, and it also causes damage to external beneficial bacteria in the human body and the natural world. Therefore, European and American countries have doubts about the safety of nanoparticles of too small size.
一般而言，將金屬銀進行奈米化而形成之奈米尺度的銀顆粒即可稱為奈米銀粒子。然而，傳統機械研磨所能形成之粒子之粒徑極限大約在500 nm左右，且藉由傳統研磨方法所形成之粒子容易具有粒徑大小不均的問題。因此，現今大都採用化學還原方法來形成奈米銀粒子。此方法為藉由將還原劑加入銀離子溶液中，使離子獲得電子而還原成金屬，而得到符合尺寸要求的奈米銀粒子。而當奈米粒子粒徑小於100 nm時，其所形成之奈米銀溶液的顏色會隨著奈米粒子濃度變高而產生變化，其中濃度越高，顏色越深。In general, nanometer-sized silver particles formed by nanocrystallization of metallic silver can be referred to as nano silver particles. However, the particle size limit of particles which can be formed by conventional mechanical polishing is about 500 nm, and the particles formed by the conventional grinding method tend to have a problem of uneven particle size. Therefore, most of todayadays chemical reduction methods are used to form nano silver particles. In this method, by adding a reducing agent to a silver ion solution, the ions are obtained by electrons and reduced to metal, thereby obtaining nano silver particles conforming to the size requirements. When the particle size of the nanoparticle is less than 100 nm, the color of the nano silver solution formed changes with the concentration of the nanoparticle, wherein the higher the concentration, the darker the color.
以異丙酮(isopropyl alcohol,IPA)為溶劑兼還原劑進行銀鹽之化學還原來合成奈米銀粒子時，由於異丙酮還原力較弱，因此通常只能合成出小於20 nm之奈米銀粒子。但小於20 nm之奈米銀粒子，可能對人體產生傷害。When isopropyl alcohol (IPA) is used as a solvent and a reducing agent to chemically reduce silver salts to synthesize nano silver particles, since the reducing power of iso-acetone is weak, it is usually only possible to synthesize nano silver particles of less than 20 nm. . However, nano silver particles smaller than 20 nm may cause harm to the human body.
因此，目前亟需一種在異丙酮系統下，形成粒徑大於30 nm的奈米銀粒子的方法。Therefore, there is a need for a method for forming nano silver particles having a particle size larger than 30 nm under an isopropanone system.
本發明提供一種奈米銀粒子的形成方法，包括：(a)混合一異丙醇、一聚乙烯吡咯烷酮與一硝酸銀以形成一反應溶液；(b)將該反應溶液加熱至低於該異丙醇的沸點的一溫度範圍以進行形成銀粒子的一反應；(c)在一促進劑存在下持續該反應；以及(d)終止該反應以使於該反應中所形成之銀粒子的平均粒徑達約50 nm-100 nm。The invention provides a method for forming nano silver particles, comprising: (a) mixing monoisopropanol, a polyvinylpyrrolidone and silver nitrate to form a reaction solution; (b) heating the reaction solution to below the isopropanium a temperature range of the boiling point of the alcohol to carry out a reaction for forming silver particles; (c) continuing the reaction in the presence of a promoter; and (d) terminating the reaction to cause an average particle of the silver particles formed in the reaction The diameter is about 50 nm-100 nm.
此外，本發明亦提供另一種奈米銀粒子的形成方法，包括：(a)提供一異丙醇、一聚乙烯吡咯烷酮與一硝酸銀以形成一反應溶液；(b)在一氣體存在下將該反應溶液加熱至低於該異丙醇的沸點的一溫度範圍以進行形成銀粒子的一反應；以及(c)終止該反應以使於該反應中所形成之銀粒子的平均粒徑達約50 nm-100 nm。In addition, the present invention also provides a method for forming another nano silver particle, comprising: (a) providing an isopropanol, a polyvinylpyrrolidone and a silver nitrate to form a reaction solution; (b) using a gas in the presence of a gas The reaction solution is heated to a temperature range lower than the boiling point of the isopropanol to perform a reaction for forming silver particles; and (c) the reaction is terminated so that the average particle diameter of the silver particles formed in the reaction is about 50 Nm-100 nm.
為了讓本發明之上述和其他目的、特徵、和優點能更明顯易懂，下文特舉較佳實施例，並配合所附圖示，作詳細說明如下：The above and other objects, features and advantages of the present invention will become more apparent from
在本發明之一態樣中，本發明提供一種奈米銀粒子的形成方法，而由此方法所形成之奈米銀粒子，其平均粒徑可達約50 nm-100 nm。In one aspect of the present invention, the present invention provides a method for forming nano silver particles, and the nano silver particles formed by the method have an average particle diameter of about 50 nm to 100 nm.
上述方法可包括，但不限於下述步驟。The above methods may include, but are not limited to, the following steps.
首先，將一異丙醇、一聚乙烯吡咯烷酮、一硝酸銀進行混合以形成一反應溶液。在一實施例中，異丙醇、聚乙烯吡咯烷酮與硝酸銀的比例可為約60-97：0.3-5.0：0.2-2.0(w/w/w)。First, monoisopropyl alcohol, polyvinylpyrrolidone, and silver nitrate are mixed to form a reaction solution. In one embodiment, the ratio of isopropanol, polyvinylpyrrolidone to silver nitrate can be from about 60 to 97:0.3 to 5.0:0.2 to 2.0 (w/w/w).
接著，將上述反應溶液加熱至低於異丙醇之沸點的一溫度範圍以進行形成銀粒子的一反應。此低於異丙醇之沸點的溫度範圍可介於約60℃至約80℃之間，較佳為介於約65℃至約78℃之間，但不限於此。而在一實施例中，係將上述反應溶液加熱至上述溫度範圍內的一設定溫度，而此設定溫度可為介於約60℃至約80℃之間的一溫度，較佳為介於約65℃至約78℃之間的一溫度。之後，在一促進劑存在下，持續上述反應。適用於此方法之促進劑可包括，但不限於，一葡萄糖、一無機鹼、一有機鹼或一氫氣。若促進劑為非氣體，則促進劑與上述反應溶液之比例可為約0.01-2：97-99(w/w)。上述作為促進劑之無機鹼的例子可為氫氧化鈉與氫氧化鉀，而作為促進劑之有機鹼，可例如胺與其類似物。在一實施例中，所使用之促進劑為葡萄糖。在另一實施例中，所使用之促進劑為氫氧化鈉。又在另一實施例中，所使用之促進劑為氫氣。Next, the above reaction solution is heated to a temperature range lower than the boiling point of isopropyl alcohol to carry out a reaction for forming silver particles. The temperature below the boiling point of the isopropanol may range from about 60 ° C to about 80 ° C, preferably from about 65 ° C to about 78 ° C, but is not limited thereto. In one embodiment, the reaction solution is heated to a set temperature within the temperature range, and the set temperature may be a temperature between about 60 ° C and about 80 ° C, preferably between about A temperature between 65 ° C and about 78 ° C. Thereafter, the above reaction is continued in the presence of a promoter. Accelerators suitable for use in this method can include, but are not limited to, monoglucose, an inorganic base, an organic base or a hydrogen. If the promoter is non-gas, the ratio of the promoter to the above reaction solution may be from about 0.01 to 2:97 to 99 (w/w). Examples of the above inorganic base as a promoter may be sodium hydroxide and potassium hydroxide, and an organic base as a promoter may be, for example, an amine or the like. In one embodiment, the accelerator used is glucose. In another embodiment, the accelerator used is sodium hydroxide. In yet another embodiment, the promoter used is hydrogen.
而於本發明方法中供應上述促進劑之時間點可如下所述：當上述反應溶液被加熱至上述低於異丙醇之沸點的溫度範圍時，就立即將促進劑供應至反應溶液。或者，在上述反應溶液被加熱至上述低於異丙醇之沸點的溫度範圍之後一段時間，才將促進劑供應至反應溶液。Further, the time at which the above accelerator is supplied in the method of the present invention can be as follows: When the above reaction solution is heated to the above temperature range lower than the boiling point of isopropyl alcohol, the promoter is immediately supplied to the reaction solution. Alternatively, the accelerator is supplied to the reaction solution only after the above reaction solution is heated to the above temperature range lower than the boiling point of the isopropanol.
然後，視需要而定，可停止促進劑的供應並持續上述反應的進行。Then, depending on the need, the supply of the promoter can be stopped and the progress of the above reaction can be continued.
於本發明中的反應溶液達到上述之溫度範圍時，即開始進行上述反應之反應時間的計算，在一實施例中，反應時間可為約5-50小時。When the reaction solution in the present invention reaches the above temperature range, the calculation of the reaction time of the above reaction is started. In one embodiment, the reaction time may be about 5 to 50 hours.
隨後，可終止上述反應以獲得平均粒徑可達約50 nm-100 nm的奈米銀粒子。終止上述反應的方式可包括，但不限於，將上述反應溶液的溫度降至室溫。在一實施例中，將一冷水或冰水添加至反應溶液使反應溶液的溫度迅速降至室溫。Subsequently, the above reaction can be terminated to obtain nano silver particles having an average particle diameter of about 50 nm to 100 nm. The manner of terminating the above reaction may include, but is not limited to, lowering the temperature of the above reaction solution to room temperature. In one embodiment, a cold water or ice water is added to the reaction solution to rapidly lower the temperature of the reaction solution to room temperature.
需注意的是，此形成奈米銀粒子的方法可適用於一放大製程。在此放大製程中，所形成之反應溶液體積適合以公升為來單位進行測量。It should be noted that this method of forming nano silver particles can be applied to an amplification process. In this amplification process, the volume of the reaction solution formed is suitably measured in units of liters.
而在本發明之另一實施態樣中，本發明也提供一種塗膜材料，其包括藉由上述之奈米銀粒子的形成方法所形成之奈米銀粒子。In still another embodiment of the present invention, the present invention also provides a coating film material comprising nano silver particles formed by the above-described method for forming nano silver particles.
此外，在本發明又另一態樣中，本發明提供另一種奈米銀粒子的形成方法，而由此方法所形成之奈米銀粒子，其平均粒徑可達約50 nm-100 nm。Further, in still another aspect of the present invention, the present invention provides a method of forming another nano silver particle, and the nano silver particles formed by the method have an average particle diameter of about 50 nm to 100 nm.
上述方法可包括，但不限於下述步驟。The above methods may include, but are not limited to, the following steps.
首先，將一異丙醇、一聚乙烯吡咯烷酮、一硝酸銀進行混合以形成一反應溶液。在一實施例中，異丙醇、聚乙烯吡咯烷酮與硝酸銀的比例可為約60-97：0.3-5.0：0.2-2.0(w/w/w)。First, monoisopropyl alcohol, polyvinylpyrrolidone, and silver nitrate are mixed to form a reaction solution. In one embodiment, the ratio of isopropanol, polyvinylpyrrolidone to silver nitrate can be from about 60 to 97:0.3 to 5.0:0.2 to 2.0 (w/w/w).
接著，在一氣體存在下，將上述反應溶液加熱至低於異丙醇之沸點的一溫度範圍以進行形成銀粒子的一反應。在一實施例中，上述反應的反應時間可為約5-25小時，但不限於此。Next, the above reaction solution is heated to a temperature range lower than the boiling point of isopropyl alcohol in the presence of a gas to carry out a reaction for forming silver particles. In one embodiment, the reaction time of the above reaction may be about 5-25 hours, but is not limited thereto.
又適用於此方法之氣體可包括，但不限於一氫氣。而上述低於異丙醇的沸點的溫度範圍可介於約60℃至約80℃之間，較佳為介於約65℃至約78℃之間，但不限於此。而一實施例中，係將上述反應溶液加熱至上述溫度範圍內的一設定溫度，而此設定溫度可為介於約60℃至約80℃之間的一溫度，較佳為介於約65℃至約78℃之間的一溫度。Gases suitable for use in this method may include, but are not limited to, a hydrogen gas. While the above temperature lower than the boiling point of the isopropanol may range from about 60 ° C to about 80 ° C, preferably from about 65 ° C to about 78 ° C, but is not limited thereto. In one embodiment, the reaction solution is heated to a set temperature within the temperature range, and the set temperature may be a temperature between about 60 ° C and about 80 ° C, preferably about 65. A temperature between °C and about 78 °C.
然後，視需要而定，可停止氣體的供應並持續上述反應的進行。在一實施例中，除上述反應時間外，在停止上述氣體的供應後，額外地使反應持續約10-20小時。隨後，可終止上述反應以獲得平均粒徑可達約50 nm-100 nm的奈米銀粒子。終止上述反應的方式可包括，但不限於，將上述反應溶液降低至室溫。在一實施例中，將一冷水或冰水添加至反應溶液使反應溶液迅速降低至室溫。Then, depending on the need, the supply of the gas can be stopped and the progress of the above reaction can be continued. In one embodiment, in addition to the above reaction time, the reaction is additionally allowed to continue for about 10-20 hours after the supply of the above gas is stopped. Subsequently, the above reaction can be terminated to obtain nano silver particles having an average particle diameter of about 50 nm to 100 nm. The manner of terminating the above reaction may include, but is not limited to, lowering the above reaction solution to room temperature. In one embodiment, a cold water or ice water is added to the reaction solution to rapidly lower the reaction solution to room temperature.
視需要而定，也可在反應終止後，使反應溶液維持於室溫一段時間。在一實施例中，在停止上述促進劑的供應並終止上述反應後，額外地使反應溶液維持於室溫約5-15小時。The reaction solution may be maintained at room temperature for a while after the reaction is terminated, as needed. In one embodiment, after the supply of the above accelerator is stopped and the above reaction is terminated, the reaction solution is additionally maintained at room temperature for about 5-15 hours.
需注意的是，此形成奈米銀粒子的方法可適用於一放大製程。在此放大製程中，所形成之反應溶液體積適合以公升為來單位進行測量。It should be noted that this method of forming nano silver particles can be applied to an amplification process. In this amplification process, the volume of the reaction solution formed is suitably measured in units of liters.
再者，在本發明又另一態樣中，本發明提供另一種奈米銀粒子的形成方法，而由此方法所形成之奈米銀粒子，其平均粒徑可達約50 nm-100 nm。Furthermore, in still another aspect of the present invention, the present invention provides another method for forming nano silver particles, and the nano silver particles formed by the method have an average particle diameter of about 50 nm to 100 nm. .
【實施例】[Examples]
1. 比較例Comparative example
(1) 奈米銀粒子之製備(1) Preparation of nano silver particles
將異丙醇(商品編號CMOS111-00000-72EC，台灣景明化工公司製造)、聚乙烯吡咯烷酮(商品編號CAS9003-39-8-85656-8，美國Sigma-Aldrich製造，分子量約為55000)與硝酸銀(商品編號CAS7761-88-82169-03，美國Mallinckrodt Chemicals製造，純度99%)均勻混合以形成一反應溶液。接著將反應溶液加熱至70℃以進行反應。當反應溶液達70℃時開始反應時間的計算。在反應時間為12、21.5、84、90小時之時對反應溶液進行取樣。比較例之詳細製備條件如下列表1所示。Isopropyl alcohol (commercial number CMOS111-00000-72EC, manufactured by Taiwan Jingming Chemical Co., Ltd.), polyvinylpyrrolidone (commercial number CAS9003-39-8-85656-8, manufactured by Sigma-Aldrich, USA, molecular weight of about 55,000) and silver nitrate Commercial product number CAS7761-88-82169-03, manufactured by Mallinckrodt Chemicals, USA, purity 99%) was uniformly mixed to form a reaction solution. The reaction solution was then heated to 70 ° C to carry out the reaction. The calculation of the reaction time was started when the reaction solution reached 70 °C. The reaction solution was sampled at a reaction time of 12, 21.5, 84, and 90 hours. The detailed preparation conditions of the comparative examples are shown in Table 1 below.
2. 實施例12. Example 1
(1) 奈米銀粒子之製備(1) Preparation of nano silver particles
將異丙醇、聚乙烯吡咯烷酮與硝酸銀均勻混合以形成一反應溶液。接著將反應溶液加熱至70℃以進行反應。當反應溶液達70℃時開始反應時間的計算。在反應時間為20小時之時加入葡萄糖(商品編號CAS492-62-6207-757-8，比利時Acros製造，純度99%)。接著在反應時間為28小時之時對反應溶液進行取樣。實施例1之詳細製備條件如下列表2所示。Isopropanol, polyvinylpyrrolidone and silver nitrate were uniformly mixed to form a reaction solution. The reaction solution was then heated to 70 ° C to carry out the reaction. The calculation of the reaction time was started when the reaction solution reached 70 °C. Glucose was added at a reaction time of 20 hours (commercial number CAS 492-62-6207-757-8, manufactured by Acros, Belgium, purity 99%). The reaction solution was then sampled at a reaction time of 28 hours. The detailed preparation conditions of Example 1 are shown in Table 2 below.
3. 實施例23. Example 2
(1) 奈米銀粒子之製備(1) Preparation of nano silver particles
將異丙醇、聚乙烯吡咯烷酮與硝酸銀均勻混合以形成一反應溶液。接著將反應溶液加熱至76.5℃以進行反應。當反應溶液達76.5℃時開始反應時間的計算。而當反應溶液達76.5℃時即加入氫氧化鈉溶液(商品編號CAS1310-73-2，美國Sigma-Aldrich製造)。接著在反應時間為18、26、40、46與49小時之時分別對反應溶液進行取樣。實施例2之詳細製備條件如下列表3所示。Isopropanol, polyvinylpyrrolidone and silver nitrate were uniformly mixed to form a reaction solution. The reaction solution was then heated to 76.5 ° C to carry out the reaction. The calculation of the reaction time was started when the reaction solution reached 76.5 °C. When the reaction solution reached 76.5 ° C, a sodium hydroxide solution (commodity number CAS1310-73-2, manufactured by Sigma-Aldrich, USA) was added. The reaction solution was then separately sampled at reaction times of 18, 26, 40, 46 and 49 hours. The detailed preparation conditions of Example 2 are shown in Table 3 below.
(2) 奈米銀粒子之反應溶液的紫外光譜(2) Ultraviolet spectrum of the reaction solution of nano silver particles
將於反應時間為6小時所取得之反應溶液樣本進行紫外光譜分析，結果顯示於第1a圖。第1a圖顯示反應溶液樣本在紫外光譜中之418 nm中具有一個波峰。由於奈米銀粒子在紫外光譜中之410 nm-435 nm之間會出現吸收光譜，因此由此可知反應溶液中具有奈米銀粒子。The sample of the reaction solution obtained at a reaction time of 6 hours was subjected to ultraviolet spectrum analysis, and the results are shown in Fig. 1a. Figure 1a shows that the sample of the reaction solution has a peak at 418 nm in the ultraviolet spectrum. Since the nano silver particles have an absorption spectrum between 410 nm and 435 nm in the ultraviolet spectrum, it is understood that the reaction solution has nano silver particles.
(3) 奈米銀粒子粒徑大小分佈(3) Particle size distribution of nano silver particles
於反應時間為18、26、40、46與49小時所取得之反應溶液樣本中之奈米銀粒子粒徑大小的分佈情況，分別顯示於第1b至1g圖。The distribution of the particle size of the nano silver particles in the reaction solution samples obtained at reaction times of 18, 26, 40, 46 and 49 hours is shown in Figures 1b to 1g, respectively.
(4) 反應溶液的顏色(4) Color of the reaction solution
目前已知奈米銀溶液的顏色會隨著奈米粒子濃度增高而變深。It is currently known that the color of the nanosilver solution becomes darker as the concentration of the nanoparticle increases.
由上述各反應溶液樣本的顏色可知，隨著反應時間延長，反應溶液的顏色由淡褐色變為深褐色再變成紅褐色，最後變成藍褐色。It can be seen from the color of each of the above reaction solution samples that as the reaction time is prolonged, the color of the reaction solution changes from light brown to dark brown to reddish brown, and finally to a blue-brown color.
4. 實施例34. Example 3
(1) 奈米銀粒子之製備(1) Preparation of nano silver particles
將異丙醇、聚乙烯吡咯烷酮與硝酸銀均勻混合以形成一反應溶液。接著將反應溶液加熱至76.5℃以進行反應。當反應溶液達76.5℃時開始反應時間的計算。在反應時間為2小時之時即提供氫氣，氫氣提供時間為約5小時。接著在反應時間為2與7小時之時分別對反應溶液進行取樣。實施例3之詳細製備條件如下列表4所示。Isopropanol, polyvinylpyrrolidone and silver nitrate were uniformly mixed to form a reaction solution. The reaction solution was then heated to 76.5 ° C to carry out the reaction. The calculation of the reaction time was started when the reaction solution reached 76.5 °C. Hydrogen was supplied at a reaction time of 2 hours, and the hydrogen supply time was about 5 hours. The reaction solution was then separately sampled at a reaction time of 2 and 7 hours. The detailed preparation conditions of Example 3 are shown in Table 4 below.
(2) 奈米銀粒子之反應溶液紫外光譜(2) Ultraviolet spectrum of reaction solution of nano silver particles
將於反應時間為7小時所取得之反應溶液樣本進行紫外光譜分析，結果顯示於第2a圖。第2a圖顯示吸收光譜出現於410 nm。The sample of the reaction solution obtained at a reaction time of 7 hours was subjected to ultraviolet spectrum analysis, and the results are shown in Fig. 2a. Figure 2a shows that the absorption spectrum appears at 410 nm.
(3) 奈米銀粒子粒徑大小分佈(3) Particle size distribution of nano silver particles
於反應時間為2與7小時所取得之反應溶液樣本中之奈米銀粒子粒徑大小的分佈情況，分別顯示於第2b至2c圖。The distribution of the particle size of the nano silver particles in the sample of the reaction solution obtained at a reaction time of 2 and 7 hours is shown in Figures 2b to 2c, respectively.
5. 實施例45. Example 4
(1) 奈米銀粒子之製備(1) Preparation of nano silver particles
將異丙醇、聚乙烯吡咯烷酮與硝酸銀均勻混合以形成一反應溶液。在氫氣存在下，將反應溶液加熱至76.5℃以進行反應。當反應溶液達76.5℃時開始反應時間的計算。在反應時間為7.5小時之時即停止氫氣供應，並於76.5℃將反應溶液持續攪拌15小時。然後立即對反應溶液進行取樣。實施例4之詳細製備條件如下列表5所示。Isopropanol, polyvinylpyrrolidone and silver nitrate were uniformly mixed to form a reaction solution. The reaction solution was heated to 76.5 ° C in the presence of hydrogen to carry out the reaction. The calculation of the reaction time was started when the reaction solution reached 76.5 °C. The hydrogen supply was stopped at a reaction time of 7.5 hours, and the reaction solution was continuously stirred at 76.5 ° C for 15 hours. The reaction solution was then immediately sampled. The detailed preparation conditions of Example 4 are shown in Table 5 below.
(2) 奈米銀粒子之反應溶液紫外光譜(2) Ultraviolet spectrum of reaction solution of nano silver particles
將於經上述步驟所取得之反應溶液樣本進行紫外光譜分析，結果顯示於第3a圖。The sample of the reaction solution obtained by the above steps was subjected to ultraviolet spectrum analysis, and the results are shown in Fig. 3a.
第3a圖顯示經上述步驟取得之反應溶液樣本在紫外光譜中出現兩個波峰，分別在425 nm與538 nm。Figure 3a shows that the sample of the reaction solution obtained by the above procedure has two peaks in the ultraviolet spectrum, at 425 nm and 538 nm, respectively.
由上述結果可得知反應溶液樣本之光譜出現第二個波峰，且光譜呈現紅位移現象，而此可能是由於於反應溶液中之奈米銀粒子粒徑變大或聚集所導致。From the above results, it can be seen that the spectrum of the sample of the reaction solution shows a second peak, and the spectrum exhibits a red shift phenomenon, which may be caused by the large particle size or aggregation of the nano silver particles in the reaction solution.
(3) 掃瞄式電子顯微鏡分析(3) Scanning electron microscope analysis
將於經上述步驟所取得之反應溶液樣本進行掃瞄式電子顯微鏡分析，結果顯示於第3b圖。第3b圖顯示奈米銀粒子粒徑大小為介於40 nm-150 nm之間。The sample of the reaction solution obtained in the above procedure was subjected to scanning electron microscope analysis, and the results are shown in Fig. 3b. Figure 3b shows that the nano silver particles have a particle size between 40 nm and 150 nm.
(4) 反應溶液的顏色(4) Color of the reaction solution
觀察所取得之反應溶液樣本得知反應溶液的顏色為桃紅色。The obtained reaction solution sample was observed to find that the color of the reaction solution was pink.
6. 實施例56. Example 5
(1) 奈米銀粒子之製備(1) Preparation of nano silver particles
將異丙醇、聚乙烯吡咯烷酮與硝酸銀均勻混合以形成一反應溶液。在氫氣存在下，將反應溶液加熱至76.5℃以進行反應。當反應溶液達76.5℃時開始反應時間的計算。在反應時間為7.5小時之時即停止氫氣供應，並將冰水添加至反應溶液，使反應溶液降低至室溫。接著將反應溶液於室溫將持續攪拌12小時。之後立即對反應溶液進行取樣。實施例5之詳細製備條件如下列表6所示。Isopropanol, polyvinylpyrrolidone and silver nitrate were uniformly mixed to form a reaction solution. The reaction solution was heated to 76.5 ° C in the presence of hydrogen to carry out the reaction. The calculation of the reaction time was started when the reaction solution reached 76.5 °C. The hydrogen supply was stopped at a reaction time of 7.5 hours, and ice water was added to the reaction solution to lower the reaction solution to room temperature. The reaction solution was then stirred at room temperature for 12 hours. Immediately thereafter, the reaction solution was sampled. The detailed preparation conditions of Example 5 are shown in Table 6 below.
(2) 奈米銀粒子粒徑大小分佈(2) Particle size distribution of nano silver particles
經上述步驟所取得之反應溶液樣本中的奈米銀粒子粒徑大小的分佈情況，顯示於第4圖。The distribution of the particle size of the nanosilver particles in the sample of the reaction solution obtained by the above procedure is shown in Fig. 4.
(3) 反應溶液的顏色(3) Color of the reaction solution
觀察所取得之反應溶液樣本得知反應溶液的顏色為黃褐色。Observation of the obtained reaction solution sample revealed that the color of the reaction solution was yellowish brown.
雖然本發明已以較佳實施例揭露如上，然其並非用以限定本發明，任何熟習此技藝者，在不脫離本發明之精神和範圍內，當可作些許之更動與潤飾，因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。While the present invention has been described in its preferred embodiments, the present invention is not intended to limit the invention, and the present invention may be modified and modified without departing from the spirit and scope of the invention. The scope of protection is subject to the definition of the scope of the patent application.
第1a圖顯示於反應時間為26小時所取得之實施例2反應溶液樣本的紫外光譜。Figure 1a shows the ultraviolet spectrum of the sample of the reaction solution of Example 2 taken at a reaction time of 26 hours.
第1b至1f圖分別顯示於反應時間為18、26、40、46與49小時所取得之實施例2反應溶液樣本中之奈米銀粒子粒徑大小的分佈情況。Figures 1b to 1f show the distribution of the particle size of the nano silver particles in the sample of the reaction solution of Example 2 obtained at reaction times of 18, 26, 40, 46 and 49 hours, respectively.
第2a圖顯示於反應時間為7小時所取得之實施例3反應溶液樣本的紫外光譜。Fig. 2a shows the ultraviolet spectrum of the sample of the reaction solution of Example 3 obtained at a reaction time of 7 hours.
第2a至2c圖分別顯示於反應時間為2與7小時所取得之實施例3反應溶液樣本中之奈米銀粒子粒徑大小的分佈情況。Figures 2a to 2c show the distribution of the particle size of the nanosilver particles in the sample of the reaction solution of Example 3 obtained at a reaction time of 2 and 7 hours, respectively.
第3a圖顯示實施例4之反應溶液樣本的紫外光譜。Figure 3a shows the ultraviolet spectrum of the sample of the reaction solution of Example 4.
第3b圖顯示實施例4之反應溶液樣本的掃瞄式電子顯微鏡圖。Figure 3b shows a scanning electron micrograph of a sample of the reaction solution of Example 4.
第4圖顯示實施例5之反應溶液樣本中之奈米銀粒子粒徑大小的分佈情況。Fig. 4 is a view showing the distribution of the particle size of the nano silver particles in the sample of the reaction solution of Example 5.
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